CN109592683B - Ultra-small vanadium carbide embedded carbon atom layer material and preparation method thereof - Google Patents

Ultra-small vanadium carbide embedded carbon atom layer material and preparation method thereof Download PDF

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CN109592683B
CN109592683B CN201910066609.1A CN201910066609A CN109592683B CN 109592683 B CN109592683 B CN 109592683B CN 201910066609 A CN201910066609 A CN 201910066609A CN 109592683 B CN109592683 B CN 109592683B
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冯亮亮
白嘉玺
黄倩
张宁
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Shaanxi University of Science and Technology
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Abstract

A material of a material with ultra-small vanadium carbide embedded into a carbon atom layer and a preparation method thereof are disclosed, wherein dicyandiamide, ammonium metavanadate and cobalt nitrate hexahydrate are mixed and fully ground to obtain a reactant raw material; placing reactant raw materials into a porcelain boat, and placing the porcelain boat in a tubular furnace under vacuum or protective atmosphere for one-step calcination to obtain black powder; placing black powder in H2SO4And drying the solution in vacuum, and grinding to obtain the vanadium carbide coated by the carbon atom layer, wherein the particle size of the vanadium carbide is less than 3nm, the crystallized carbon atom layer is 5-10 layers, the appearance is uniform, and the dispersion is good. The VC @ CL hydrogen production electrocatalyst has the advantages of short reaction period, uniform material chemical composition, uniform appearance and size, high electrocatalytic activity in acid-base electrolyte and high stability by adopting a calcination method. The cobalt nitrate hexahydrate in the reactant raw material not only promotes the crystallization of the carbon layer, but also inhibits the growth of VC grains, so that ultra-small VC particles (not more than 3nm) are generated.

Description

Ultra-small vanadium carbide embedded carbon atom layer material and preparation method thereof
Technical Field
The invention relates to the technical field of synthesis and application of catalysts, in particular to a material of an ultra-small vanadium carbide embedded carbon atom layer and a preparation method thereof.
Background
With the aggravation of energy problems, the human society has an increasing demand for energy, and hydrogen energy has received wide attention as a new generation of clean sustainable energy, and meanwhile, the development of hydrogen is promoted. The hydrogen production by water splitting is a high-efficiency hydrogen production means, so the development of a high-efficiency hydrogen production catalyst is the key of the technology. Platinum-based catalysts are considered to be the most efficient hydrogen production catalysts, but their high cost and low content limit their industrial application. Therefore, there is a need to find non-noble metal electrocatalysts, including transition metal carbides, sulfides, nitrides, phosphides, etc., that can replace platinum-based catalysts. Among transition metal carbides, the cheaper VC has excellent hydrogen adsorption properties, and Mo2C is more than WCThe small density makes it more suitable as a catalyst. However, due to its high synthesis temperature and uncontrollable morphology, VC has been rarely studied as a catalyst, particularly for applications in water splitting to produce hydrogen and oxygen. Therefore, the development of the vanadium carbide water-splitting hydrogen production electrocatalyst is also a piece of work with challenges and significance.
The research of the literature of about 15 years proves that the exploration of the vanadium carbide material in China mainly focuses on the field of the preparation of the metal ceramic material, the synthesis process is various, but the research is different, the research can be basically summarized into a calcination method, a carbon source and a vanadium source are adopted, and the vanadium carbide material is sintered in a high-temperature furnace with or without an auxiliary agent, the sintering process of the material prepared by the method is easy to agglomerate, the grain diameter is difficult to refine, the grain diameter of the vanadium carbide prepared at present in China is 50nm at the minimum, the vanadium carbide is mostly used in the field of the metal ceramic material, and the requirement of an electrocatalyst.
Disclosure of Invention
The invention aims to provide a material with ultra-small vanadium carbide embedded carbon atoms, which has the advantages of short reaction period, uniform material chemical composition and uniform appearance and size, and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the method comprises the following steps: dicyandiamide, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the weight ratio of (65-90): 1: (9-12) mixing and fully grinding the raw materials in a mass ratio to obtain a reactant raw material;
step two: placing reactant raw materials in a porcelain boat, placing the porcelain boat in a tubular furnace under vacuum or protective atmosphere, heating the reactant raw materials from room temperature to 500-1200 ℃ at the heating rate of 5-10 ℃/min, and preserving heat for 1-5h to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4And after 10-24h, carrying out vacuum drying and grinding to obtain the material of the ultra-small vanadium carbide embedded carbon atom layer.
And the protective atmosphere in the second step is argon or nitrogen.
The ultra-small vanadium carbide embedded carbon atom layer material prepared by the preparation method is characterized in that: the vanadium carbide coated by the carbon atom layer has the particle size of less than 3nm, 5-10 crystallized carbon atom layers, uniform appearance and good dispersibility.
The invention takes dicyandiamide as a carbon source, ammonium metavanadate as a vanadium source, cobalt nitrate hexahydrate as a catalyst, and prepares the material of the ultra-small vanadium carbide embedded carbon atom layer by a one-step calcination method to be used as a hydrogen production electrocatalyst for water cracking, and the material has excellent hydrogen production activity and good stability within the pH range of 0-14. The VC @ CL hydrogen production electrocatalyst has the advantages of short reaction period, uniform material chemical composition, uniform appearance and size, high electrocatalytic activity in acid-base electrolyte and high stability by adopting a calcination method. The cobalt nitrate hexahydrate in the reactant raw material not only promotes the crystallization of the carbon layer, but also inhibits the growth of VC grains, so that ultra-small VC particles (not more than 3nm) are generated.
Compared with the prior art, the invention has the following beneficial technical effects:
1) the sintering method used in the invention has simple process and short time consumption, and overcomes the defect of complicated steps in the traditional method for preparing vanadium carbide;
2) the dicyandiamide is rich in N element, so that the doping content of the prepared VC @ CL N is high, and the activity of the catalyst is improved;
3) the introduction of cobalt atoms in the raw materials is the key for generating the structure and contributes to excellent activity to a certain extent;
4) the VC @ CL hydrogen production electrocatalyst obtained through the reaction has the VC particle size of less than 3nm, 5-10 layers of surrounding carbon atom layers, uniform appearance and good dispersibility;
5) the VC @ CL hydrogen production electrocatalyst prepared by the method can be applied to a water-splitting full-pH-value hydrogen production electrocatalyst in the field of electrocatalysis.
Drawings
FIG. 1 is an XRD pattern of VC @ CL prepared in example 1 of the invention;
FIG. 2 is a TEM image of VC @ CL prepared in example 3 of the present invention;
FIG. 3 is a LSV graph of VC @ CL prepared in example 4 of the invention;
FIG. 4 is a graph of i-t for VC @ CL prepared in example 5 of the invention.
Detailed Description
The invention is further described in detail below with reference to the drawings and the embodiments.
Example 1:
the method comprises the following steps: 1.625g of dicyandiamide, 0.025g of ammonium metavanadate and 0.225g of cobalt nitrate hexahydrate are mixed and fully ground to obtain a reactant raw material;
step two: placing the reactant raw materials in a porcelain boat, placing the porcelain boat in a tubular furnace under argon atmosphere, heating the reactant raw materials from room temperature to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 4h to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4And after 10h, drying in vacuum and grinding to obtain the material (VC @ CL hydrogen production electrocatalyst) of the ultra-small vanadium carbide embedded carbon atom layer.
As can be seen from fig. 1, the number of VC standard PDF card corresponding to the prepared ultra-small vanadium carbide embedded carbon atom layer material (VC @ CL hydrogen production electrocatalyst) is 73-0476, four diffraction peaks respectively correspond to crystal planes (111), (200), (220) and (311), the diffraction peaks are sharp, and the intensity is high, which indicates that the vanadium carbide obtained in this example has good crystallinity, cobalt is cobalt embedded in the carbon layer (cobalt species coated by the carbon-free layer is dissolved and removed by acid), and carbon is graphitized carbon.
Example 2:
the method comprises the following steps: 1.625g of dicyandiamide, 0.025g of ammonium metavanadate and 0.3g of cobalt nitrate hexahydrate are mixed and fully ground to obtain a reactant raw material;
step two: placing the reactant raw materials in a porcelain boat, placing the porcelain boat in a tubular furnace under argon atmosphere, heating the reactant raw materials from room temperature to 500 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 2h to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4And after 15h, drying in vacuum and grinding to obtain the material (VC @ CL hydrogen production electrocatalyst) of the ultra-small vanadium carbide embedded carbon atom layer.
Example 3:
the method comprises the following steps: mixing 2g of dicyandiamide, 0.025g of ammonium metavanadate and 0.25g of cobalt nitrate hexahydrate, and fully grinding to obtain a reactant raw material;
step two: placing reactant raw materials into a porcelain boat, placing the porcelain boat in a tubular furnace under nitrogen atmosphere, heating the reactant raw materials from room temperature to 1000 ℃ at the heating rate of 7 ℃/min, and keeping the temperature for 1h to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4After 20h, the mixture is dried in vacuum and ground to obtain the material (VC @ CL hydrogen production electrocatalyst) of the ultra-small vanadium carbide embedded carbon atom layer.
It can be seen from fig. 2 that the microstructure of the prepared ultra-small vanadium carbide embedded carbon atom layer material (VC @ CL hydrogen production electrocatalyst) is vanadium carbide coated by a carbon atom layer, the particle size of the vanadium carbide is less than 3nm, the crystal face mainly exposed by the crystal face spacing is calculated to be (200), 5-10 layers of the coated carbon layer have obvious lattice stripes, which are indicated as graphite carbon, and are consistent with the XRD result.
Example 4:
the method comprises the following steps: mixing 2.25g of dicyandiamide, 0.025g of ammonium metavanadate and 0.225g of cobalt nitrate hexahydrate, and fully grinding to obtain a reactant raw material;
step two: placing reactant raw materials into a porcelain boat, placing the porcelain boat in a tubular furnace under nitrogen atmosphere, heating the reactant raw materials from room temperature to 1200 ℃ at the heating rate of 8 ℃/min, and preserving the heat for 5 hours to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4After 24h, the mixture is dried in vacuum and ground to obtain the material (VC @ CL hydrogen production electrocatalyst) of the ultra-small vanadium carbide embedded carbon atom layer.
FIG. 3 is a LSV plot of the VC @ CL electrocatalyst prepared in this example, showing the current density at 10mA/cm under pH 7 test conditions2When the scanning rate is 3mV/s, the overpotential of the sample is 242mV, which shows that the catalytic hydrogen production activity is excellent.
Example 5:
the method comprises the following steps: mixing 2.25g of dicyandiamide, 0.025g of ammonium metavanadate and 0.3g of cobalt nitrate hexahydrate, and fully grinding to obtain a reactant raw material;
step two: placing reactant raw materials into a porcelain boat, placing the porcelain boat into a tubular furnace under vacuum atmosphere, heating the reactant raw materials from room temperature to 900 ℃ at the heating rate of 10 ℃/min, and preserving heat for 3h to obtain black powder;
step three: will be provided withBlack powder is put in H of 0.5mol/L2SO4After 20h, the mixture is dried in vacuum and ground to obtain the material (VC @ CL hydrogen production electrocatalyst) of the ultra-small vanadium carbide embedded carbon atom layer.
FIG. 4 is a plot of i-t for the VC @ CL electrocatalyst prepared in this example, showing a current density of about 5mA/cm at an overpotential of 150mV under pH 0 test conditions2And the stability is at least 10h, the current density is not obviously attenuated, and the sample stability is excellent.
Example 6:
the method comprises the following steps: 1.75g of dicyandiamide, 0.025g of ammonium metavanadate and 0.275g of cobalt nitrate hexahydrate are mixed and fully ground to obtain a reactant raw material;
step two: placing reactant raw materials into a porcelain boat, placing the porcelain boat in a tubular furnace under argon atmosphere, heating the reactant raw materials from room temperature to 600 ℃ at the heating rate of 6 ℃/min, and keeping the temperature for 4h to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4And after 18h, drying in vacuum and grinding to obtain the material (VC @ CL hydrogen production electrocatalyst) of the ultra-small vanadium carbide embedded carbon atom layer.
Example 7:
the method comprises the following steps: mixing 2.125g of dicyandiamide, 0.025g of ammonium metavanadate and 0.2625g of cobalt nitrate hexahydrate, and fully grinding to obtain a reactant raw material;
step two: placing reactant raw materials into a porcelain boat, placing the porcelain boat in a tubular furnace under nitrogen atmosphere, heating the reactant raw materials from room temperature to 1100 ℃ at the heating rate of 9 ℃/min, and keeping the temperature for 2h to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4And after 13h, drying in vacuum and grinding to obtain the material (VC @ CL hydrogen production electrocatalyst) of the ultra-small vanadium carbide embedded carbon atom layer.
Example 8:
the method comprises the following steps: 1.875g of dicyandiamide, 0.025g of ammonium metavanadate and 0.2375g of cobalt nitrate hexahydrate are mixed and fully ground to obtain a reactant raw material;
step two: placing reactant raw materials into a porcelain boat, placing the porcelain boat into a tubular furnace under vacuum atmosphere, heating the reactant raw materials from room temperature to 1200 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1h to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4After 22h, the mixture is dried in vacuum and ground to obtain the material (VC @ CL hydrogen production electrocatalyst) of the ultra-small vanadium carbide embedded carbon atom layer.

Claims (3)

1. A preparation method of a material with ultra-small vanadium carbide embedded in a carbon atom layer is characterized by comprising the following steps:
the method comprises the following steps: dicyandiamide, ammonium metavanadate and cobalt nitrate hexahydrate are mixed according to the weight ratio of (65-90): 1: (9-12) mixing and fully grinding the raw materials in a mass ratio to obtain a reactant raw material;
step two: placing reactant raw materials in a porcelain boat, placing the porcelain boat in a tubular furnace under vacuum or protective atmosphere, heating the reactant raw materials from room temperature to 500-1200 ℃ at the heating rate of 5-10 ℃/min, and preserving heat for 1-5h to obtain black powder;
step three: putting black powder into 0.5mol/L H2SO4And after 10-24h, carrying out vacuum drying and grinding to obtain the material of the ultra-small vanadium carbide embedded carbon atom layer.
2. The method for preparing the material with the ultra-small vanadium carbide embedded in the carbon atomic layer according to claim 1, is characterized in that: and the protective atmosphere in the second step is argon or nitrogen.
3. The preparation method of claim 1, wherein the preparation method comprises the following steps: the vanadium carbide coated by the carbon atom layer has the particle size of less than 3nm, 5-10 crystallized carbon atom layers, uniform appearance and good dispersibility.
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